Trifluoroacetic acid → HCID 67173930、化合物

関与物質

反応手順

(R)-tert-butyl 2-((2-(2,6-difluoro-4-(methylcarbamoyl)phenyl)-5-methyl-1H-benzo[d]imidazol-1-yl)methyl)morpholine-4-carboxylate (770 mg, 1.54 mmol) was dissolved in DCM (10.0 mL). Afterward, TFA (2.00 mL) was added to the mixture at 0° C. The resulting mixture was stirred at room temperature for 1 hr and then concentrated under reduced pressure. The crude (S)-3,5-difluoro-N-methyl-4-(5-methyl-1-(morpholin-2-ylmethyl)-1H-benzo[d]imidazol-2-yl)benzamide trifluoroacetic acid salt product was used without further purification (790 mg) in the next step. It was analyzed on analytical HPLC MS using the high pH gradient method (mobile phase: 5-95% B; A: H2O with 10 mM NH4CO3 and 0.375% NH4OH v/v; B: CH3CN; 2.25 min run; X-Bridge C18; column size: 2.1×30 mm; particle size: 5 μm). MS m/z 401.3 [M+H]+ (ESI), Rt 1.37 min.

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